HRID650907

反应详情

EQUATION

反应方程式

HRID 650907 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This compound was prepared in a manner analogous to the second part of Step D, Example 1. Here, 16.7 grams (0.074 mole) of methyl 6-chloro-3-isocyanato-2-methylbenzoate was combined with 4.4 grams (0.110 mole) of 60% sodium hydride and 14.2 grams (0.076 mole) of 3-amino-4,4,4-trifluoro-2-butenoate in 600 mL of THF. The reaction product was purified by column chromatography on silica using a 1:1 mixture of EtOAc and hexane as eluant. The fractions containing product were combined and concentrated under reduced pressure, yielding 15.8 grams of subject compound. The NMR spectrum was consistent with the proposed structure.

WORKUP

后处理

  1. customThis compound was prepared in a manner analogous to the second part of Step D, Example 1
  2. customThe reaction product was purified by column chromatography on silica using
  3. additiona 1:1 mixture of EtOAc and hexane as eluant
  4. additionThe fractions containing product
  5. concentrationconcentrated under reduced pressure